EP1434663A2 - Verfahren zur herstellung von porösen gesinterten formkörpern - Google Patents

Verfahren zur herstellung von porösen gesinterten formkörpern

Info

Publication number
EP1434663A2
EP1434663A2 EP02782822A EP02782822A EP1434663A2 EP 1434663 A2 EP1434663 A2 EP 1434663A2 EP 02782822 A EP02782822 A EP 02782822A EP 02782822 A EP02782822 A EP 02782822A EP 1434663 A2 EP1434663 A2 EP 1434663A2
Authority
EP
European Patent Office
Prior art keywords
powder
porous
basic body
mixed crystals
nickel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP02782822A
Other languages
English (en)
French (fr)
Other versions
EP1434663B1 (de
Inventor
Alexander BÖHM
Hartmut GÖHLER
Dirk Naumann
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Vale Canada Ltd
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Original Assignee
Vale Canada Ltd
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Vale Canada Ltd, Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV filed Critical Vale Canada Ltd
Publication of EP1434663A2 publication Critical patent/EP1434663A2/de
Application granted granted Critical
Publication of EP1434663B1 publication Critical patent/EP1434663B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2027—Metallic material
    • B01D39/2031—Metallic material the material being particulate
    • B01D39/2034—Metallic material the material being particulate sintered or bonded by inorganic agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
    • B22F3/1137—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers by coating porous removable preforms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • B22F3/114—Making porous workpieces or articles the porous products being formed by impregnation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/002—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12014—All metal or with adjacent metals having metal particles
    • Y10T428/12028—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, etc.]
    • Y10T428/12042—Porous component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12014—All metal or with adjacent metals having metal particles
    • Y10T428/12028—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, etc.]
    • Y10T428/12049—Nonmetal component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12014—All metal or with adjacent metals having metal particles
    • Y10T428/12153—Interconnected void structure [e.g., permeable, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12479—Porous [e.g., foamed, spongy, cracked, etc.]

Definitions

  • the invention relates to a process for the production of sintered porous bodies and to porous bodies produced by the process and to their use.
  • Porous bodies of this type can, in contrast to metal foams which are known per se, also be employed at elevated temperatures, even up to above 1800°C, which is also desired for use as filters or catalyst supports for various applications.
  • Bodies or elements of this type are also desired for use as lightweight thermal insulation elements, where upper temperature limits and chemically aggressive, corrosion-promoting ambient conditions frequently prevent use.
  • the object of the invention is therefore to propose a process for the production of sintered porous bodies which achieve improved properties, such as an increased surface area of such bodies, deformability of the structures ' at room temperature or modification of the initial pore volume.
  • a sintered porous body produced in accordance with the invention has intermetallic phases or mixed crystals in surface regions, i.e. also within the pore structure, or is formed entirely of these intermetallic phases or mixed crystals. In the former case, it is not necessary to coat the entire surface with intermetallic phases or mixed crystals. It is also possible for certain surface regions to be selected and correspondingly modified in a targeted manner, enabling chemical and physical properties also to be correspondingly influenced locally.
  • the porosity is essentially determined by a porous basic body likewise used in the production which serves as support for the elements forming the intermetallic phases or mixed crystals.
  • elements forming intermetallic phases or mixed crystals are applied to and introduced into the structure, as will be explained in greater detail below, and the phases or mixed crystals are formed by means of heat treatment, with the pore size generally being reduced compared with the initial pore size of the basic structure used in each case, but the overall effective surface area is increased.
  • the porosity of the bodies is in the range from 70 to 99.5% of the theoretical density.
  • the intermetallic phases or mixed crystals can be formed from at least two elements selected from nickel, iron, titanium, cobalt, aluminum, copper, silicon, molybdenum or tungsten. However, preference is given to aluminides or suicides, with nickel aluminides being particularly preferred. Thus, for example, nickel aluminide can be formed on a porous nickel basic structure, it being possible for the nickel basic structure to form a ductile core.
  • These elements can be employed as powders, and the intermetallic phase or the mixed crystals can then be formed with the basic body material. However, it is also possible to employ powder mixtures with elements which form phases or crystals of this type.
  • a powder mixture may also additionally comprise elements which form alloys (for example Cr, Ta, Nb, Bi, Sn or Zn) in an amount of up to 20% by weight .
  • reinforcing components are integrated into a porous body or embedded in a surface coating.
  • Reinforcing components of this type are, for example, SiC, Zr0 2 , A1 2 0 3 , TiB 2 and/or Hf0 2 . These can be applied with the components forming intermetallic phases or mixed crystals before the heat treatment or alternatively formed reactively before, during or after the heat treatment for the formation of the intermetallic phases or mixed crystals. In this way, it is also possible to incorporate functional components, which influence, for example, the oxidation behavior.
  • 03/033192 are, for example, SiC, Zr0 2 , A1 2 0 3 , TiB 2 and/or Hf0 2 .
  • a porous body according to the invention may have a single intermetallic phase or alternatively more than one intermetallic phase or one or more different mixed crystals.
  • a possible procedure in the production is that a suspension/dispersion comprising at least sintering- active powder which forms an intermetallic phase or a mixed crystal is applied to a porous basic body.
  • the reaction for the formation of the intermetallic phases or the mixed crystals can be carried out later between the powders of the dispersion with one another or between the powder and the basic substrate.
  • This can be followed by drying, which can in turn be followed by heat treatment for the formation of at least one intermetallic phase or mixed-crystal form, with a possible increase in the specific surface area being carried out at the same time.
  • the heat treatment should always be carried out at temperatures which are suitable for the sintering of a powder or powder mixture.
  • the suspension/dispersion may additionally comprise organic and/or inorganic binders.
  • the suspension/dispersion comprises an organic binder and/or a basic body comprising an organic porous material, for example elamine or PUR foam has been used, the organic constituents should be expelled before this heat treatment, which can readily be achieved by means of interim heating (pyrolysis) at temperatures not exceeding 750°C and generally below.
  • Particularly sintering-active powders or powder mixtures comprising elements which form intermetallic phases enable a significant lowering of the requisite sintering temperatures, enabling intermetallic phases of elements which actually require significantly higher sintering temperatures also to be obtained on porous bodies produced in accordance with the invention.
  • the temperatures necessary for this purpose can be reduced down to 500°C, which is several 100° below the actual temperatures • required.
  • sintering and titanium aluminide formation can be carried out at a temperature of only about 500°C.
  • sintering-active powders of this type can also be obtained by modified grinding methods or coating methods.
  • the powders to be used are advantageously subjected to a high-energy grinding process, in which the elements of the powder or powder mixture adopt the form of fine lamellae and phase formations should be avoided.
  • a powder or powder mixture of this type can also be applied directly to surfaces of a porous basic body without carrying out the preparation of a suspension/dispersion, and the intermetallic phases or mixed crystals can be formed during the heat treatment, without the need for drying.
  • a change in the surface energy or interfacial tension may be favorable. This can be achieved, for example, by physico-chemical processes known per se. If powders are applied alone, electrostatic charging, for example of the basic body, may be advantageous .
  • the interfacial tension between the surface of the basic body can be influenced, for example, by means of a suitable agent, which can be added to the suspension/dispersion.
  • a suitable agent which can be added to the suspension/dispersion.
  • This can be, for example, a surfactant, with which the wettability can be improved.
  • intermetallic phases can be formed with aluminum or silicon powder if a metallic porous basic body; for example of nickel or molybdenum, is used.
  • the basic body can also be formed from other metals which correspond to the suitable powders mentioned above.
  • mixtures of powders of this type which are at least two different elements, preferably by means of a suspension/dispersion, and which form intermetallic phases or mixed crystals .
  • the starting powders should be finely ground, wherever possible under inert ambient conditions (for example argon) , so that the mean particle size (d50) is less than 0.15 mm, preferably less than 0.05 mm. Use is preferably made for this purpose of a high-energy grinding process which excludes extensive phase formation during the grinding.
  • the suspension/dispersion essentially formed from water and comprising sintering/active powders or powder mixtures prepared in this way can then be applied to the porous basic body, which can be carried out by dipping, spraying, or by means of pressure support. In the latter case, the suspension/dispersion can be pressed into the porous basic body or sucked through it.
  • the suspension/dispersion may additionally also comprise organic binders.
  • the density and porosity of the finished body can be influenced, in particular, through the type and manner of powder application. It is possible to set gradients of these parameters in which different densities, pore sizes and/or porosities occur at the surface, in the region close to the surface and in the interior of the bodies .
  • the pores of the basic body can be filled at least partially with a powder or powder mixture, and the intermetallic phase or mixed crystals can subsequently be formed.
  • porous particles which increase the specific surface area to be formed in the pores .
  • the adhesion of a powder or powder mixture can be improved for application to a porous basic body. This enables losses to be reduced.
  • magnetization can be carried out with the aid of correspondingly suitable permanent magnets or also electromagnets.
  • Magnetization of this type can be carried out here on a porous basic body whose material has ferromagnetic properties, as is the case, for example, in a porous basic body made of nickel.
  • magnetization of a powder or powder mixture can in the same form also result in the same effect, with at least one constituent in the powder having ferromagnetic properties of this type in this case.
  • both basic bodies and powders can be magnetized correspondingly, enabling an additionally increased attractive force and correspondingly improved adhesion of the powder to be ensured before the sintering.
  • electrostatic charging can also be carried out in similar form, which in turn can likewise be achieved merely on the basic body or the powder or powder mixture or on both with opposite polarity.
  • electrostatic charging can also be carried out on porous basic bodies, powders or powder mixtures, with in this case no requirements regarding ferromagnetic properties being made, but instead it even being possible for porous basic bodies made from organic materials to be electrostatically charged in a corresponding manner.
  • intermetallic phases or mixed crystals can also be applied to a porous basic body as temporary liquid phase and the intermetallic phases or mixed crystals can be formed by heat treatment.
  • the formation of liquid phases is also possible for a short time during sintering.
  • aluminum is in molten form at a temperature of only about 660°C and can thus form nickel aluminide with nickel.
  • a powder mixture can comprise at least two elements having melting points which differ by up to about 500°K from one another, i.e. an element of relatively low melting point and an element of relatively high melting point.
  • Intermetallic phases or mixed crystals can only be formed here by the element having the relatively low melting point, where appropriate during passage through a temporary liquid phase, and the element having the relatively high melting point can merely be sintered.
  • a suspension/dispersion of water with 3% by weight of polyvinylpyrrolidone as organic binder was prepared using the powder mixture prepared in this way.
  • a binder/solids ratio of 3:100 was set in the dispersion.
  • the heat treatment for the formation of nickel aluminide as intermetallic phase on the surface of the nickel basic body was carried out at 1000°C under argon for a period of 1 hour.
  • a porous PUR basic body was dipped into a suspension in accordance with Example 1, subsequently dried and then subjected to two-stage heat treatment .
  • the organic constituents were removed at a temperature of about 450°C. This was carried out over a period of 30 minutes.
  • the temperature was increased to 1030°C and work was carried out in a hydrogen atmosphere. After a period of 1 hour, the porous body formed exclusively from nickel aluminide was cooled.
  • the suspension used here and the porous basic body correspond to Example 1.
  • the suspension was merely sprayed on all sides onto the surface of the porous basic body consisting of nickel using so-called wet powder spraying.

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Geology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Powder Metallurgy (AREA)
  • Catalysts (AREA)
  • Porous Artificial Stone Or Porous Ceramic Products (AREA)
EP02782822A 2001-10-11 2002-10-04 Verfahren zur herstellung von porösen gesinterten formkörpern Expired - Lifetime EP1434663B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10150948 2001-10-11
DE10150948A DE10150948C1 (de) 2001-10-11 2001-10-11 Verfahren zur Herstellung gesinterter poröser Körper
PCT/EP2002/011111 WO2003033192A2 (en) 2001-10-11 2002-10-04 Process for the production of sintered porous bodies

Publications (2)

Publication Number Publication Date
EP1434663A2 true EP1434663A2 (de) 2004-07-07
EP1434663B1 EP1434663B1 (de) 2007-09-12

Family

ID=7702618

Family Applications (1)

Application Number Title Priority Date Filing Date
EP02782822A Expired - Lifetime EP1434663B1 (de) 2001-10-11 2002-10-04 Verfahren zur herstellung von porösen gesinterten formkörpern

Country Status (10)

Country Link
US (1) US6926969B2 (de)
EP (1) EP1434663B1 (de)
JP (1) JP4064348B2 (de)
KR (1) KR100578178B1 (de)
CN (2) CN101585084B (de)
AT (1) ATE372846T1 (de)
CA (1) CA2444931C (de)
DE (2) DE10150948C1 (de)
TW (1) TWI257334B (de)
WO (1) WO2003033192A2 (de)

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CA2444931C (en) 2009-09-22
DE60222448T2 (de) 2008-06-12
DE10150948C1 (de) 2003-05-28
EP1434663B1 (de) 2007-09-12
CN101585084A (zh) 2009-11-25
JP2005505693A (ja) 2005-02-24
DE60222448D1 (de) 2007-10-25
CA2444931A1 (en) 2003-04-24
US6926969B2 (en) 2005-08-09
ATE372846T1 (de) 2007-09-15
US20040101706A1 (en) 2004-05-27
KR20040028748A (ko) 2004-04-03
TWI257334B (en) 2006-07-01
WO2003033192A3 (en) 2003-09-04
WO2003033192A2 (en) 2003-04-24
JP4064348B2 (ja) 2008-03-19
CN101585084B (zh) 2012-06-27
CN1514756A (zh) 2004-07-21

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